2D solid state homonuclear and heteronuclear correlation experiments to study a new pharmaceutical compound

Y. GARRO LINCK; A.K CHATTAH; C. ROMAÑUK; M.E. OLIVERA; R.H. MANZO; S.L. CUFFINI; R. GRAF; G.A. MONTI; H.W. SPIESS

Göteborg

Conferencia; EUROMAR Magnetic Resonance Conference; 2009

In this work we have performed 2D 13C-1H heteronuclear correlation experiments (REPT-HSQC and HETCOR) which allowed the complete assignment of the resolved 1H solid state spectrum.[Schnell et al. J. Mag. Reson. 150, 57?70 (2001) and van Rossum et al. J. Mag. Reson. 124, 516?519 (1997)] These data were complemented with double quantum MAS experiments (BABA pulse sequence [Schnell et al. J. Mag. Reson. 133, 61-69 (1998)]) to identify 1H-1H connectivities, hydrogen bonds and dipolar proximities. The zwitterionic character of ciprofloxacin and its derivative was identified. Further information about inter and intra molecular interactions in both solid forms of the new saccharinate was obtained. Differences and similarities in the structures of the different solid forms have also been established and supported with single crystal XR diffraction data obtained for CIP-SAC (II).